Concentrated perfume compositions and manufacture of fabric softening compositions therefrom

ABSTRACT

The invention provides liquid compositions comprising: (a) 15-95 wt % lipophilic perfume. (b) 0.05-5 wt % water-soluble dye, (c) 4-50 wt % of a stabilising agent comprising a cationic stabilising agent, and (d) water miscible solvent wherein the composition comprises between 0.1 to 20 wt % water, the cationic stabilising agent has an Lα to Lβ transition temperature of 45° C. or less for a 5 wt % dispersion of the stabilising agent in water, and the solvent is present in an amount of up to 10 wt %. These concentrated perfume and dye compositions find particular application in fabric softening compositions. Also provided is a method of preparing a fabric conditioning composition by preparing a base composition comprising a cationic and/or nonionic fabric softening agent, and adding thereto, a composition of the invention. The fabric conditioning compositions thus produced are also provided. Simplified automated manufacture of fabric softening compositions is achieved.

TECHNICAL FIELD

The present invention relates to concentrated perfume compositions. Theinvention further relates to a method of manufacturing a fabricsoftening composition from the concentrated perfume composition, and, toa fabric softening composition so produced.

BACKGROUND AND PRIOR ART

In the commercial manufacture of fabric softening compositions theaccurate dosing of minor ingredients e.g. dyes, perfumes etc. is oftenproblematic because of the low levels of these ingredients required inthe compositions so that the relative proportions of these minoringredients are difficult to control. Also when compositions areproduced in batches this requires that the exact levels of minoringredients, particularly dye and perfume, must be added individuallywhich increases the possibility of inaccurate dosing.

It is also known that concentrated perfume compositions are prone toinstability problems.

Thus there is a need to provide stable concentrated compositions ofwell-known minor ingredients such as dyes and perfumes for use in themanufacture of coloured and perfumed compositions such as fabricsoftening compositions.

WO 98/08927 (Colgate-Palmolive Company) discloses colour/perfumeconcentrate compositions comprising 0.01% to 85% by weight of a polymerbound water soluble azo dye, 99.95% to 15% by weight of a perfume and 0to 99.99% by weight of a nonionic surfactant or an ethoxylated glyceroltype compound.

WO 00/06690 (Colgate-Palmolive Company), published 10 February 2000,discloses a water-in-oil microemulsion which is capable of being mixedwith an aqueous fabric softener base composition and which comprises 5to 80% by weight of a surfactant fabric softener, a solvent, perfume andcolourant.

EP 922 755 (Procter & Gamble) discloses compositions wherein alcoholethoxylates are used to solubilise dye.

U.S. Pat. No. 5,447,644 (IFF Inc.) discloses a method of controlling theviscosity of fabric softening compositions to improve shelf life byfirst forming a micro-emulsion of perfume and surfactant.

The present invention seeks to address the above problems and to providea stable concentrated composition which comprises at least two minoringredients found in fabric softening compositions at higher levels thanare typically used in a consumer product.

DEFINITION OF THE INVENTION

Accordingly the present invention provides a liquid compositioncomprising;

(a) 15-95 wt % lipophilic perfume,

(b) 0.05-5 wt % water-soluble dye,

(c) 4-50 wt % of stabilising agent comprising a cationic stabilisingagent, and

(d) water-miscible solvent,

wherein the composition comprises between 0.1 to 20 wt % water, and thecationic stabilising agent has an Lα to Lβ transition temperature of 45°C. or below for a 5% wt dispersion of the stabilising agent in water,and the solvent is present in an amount of up to 10 wt %.

All percentages by weight herein refer to the percentage based on thetotal amount of the composition.

The invention also provides a method of preparing a fabric softeningcomposition comprising the steps;

(i) preparing a base composition comprising a cationic and/or nonionicfabric softening agent, and

(ii) adding to (i) a composition as defined above to produce the fabricsoftening composition.

Furthermore the invention also provides a fabric softening compositionobtainable by the method above.

The invention provides a concentrated perfume-containing compositionthat also contains dye, both in a much higher concentration than wouldtypically be found in a fabric softening composition. This provides astable pre-mix of minor ingredients (perfume and dye). Which can beprepared at suitable ratios for direct dosage into a base composition.Excellent accuracy of the dosage of these minor ingredients into a basecomposition is achieved and this thus simplifies automated preparationof fabric softening compositions.

Furthermore the concentrated perfume and dye compositions allow accuratedosing of these minor ingredients to a base composition at a late stage(eg. after the main active ingredients have been mixed) of themanufacture of a fabric softening composition. This in turn allows awide range of compositions to be prepared from a pre-compounded basecomposition, so providing easier and more versatile manufacture. Thuschanging between variant formulations is simplified as only a small partof the automated production apparatus requires cleaning when the‘minors’ are changed in the composition (as a single ‘minor’ compositioncan be used in the process). This provides reduced aqueous effluent,saves production time and provides increased production flexibility.

In particular, the invention provides the preparation of a concentratedcomposition of perfume and dye, wherein the perfume and dye are ofdifferent lipophilic and lipophobic characters.

DETAILED DESCRIPTION OF THE INVENTION

The composition of the invention is preferably an isotropic liquid, mostpreferably a microemulsion, and especially a water-in-oil microemulsion.

It is preferred that if the composition is an isotropic liquid it doesnot contain liquid crystalline phases.

Where the compositions are not clear, they should be stable to storageat 20° C. for several days eg. 2 days. Whilst some degree of cloudinesscan be tolerated in the compositions, it is preferred that they areisotropic liquids. Such isotropic liquids may have included thereinminor amounts of materials that are not isotropic, provided, thestability of the composition is not adversely affected.

Perfume

The perfume used in the invention is lipophilic in nature. By alipophilic perfume is meant that the perfume has a solubility in water(i.e. it dissolves) of 1 g or less in 100 ml of water at 20° C.Preferably the solubility in water is equal to or less than 0.5 g,preferably equal to or less than 0.3 g in 100 ml of water at 20° C. Suchperfumes may be referred to as water-insoluble perfumes.

The perfume may be any conventional perfume used in fabric softeningcompositions. The perfume will thus preferably be compatible with thefabric softening actives typically found in fabric softeningcompositions, although, not many commercially available perfumes willnot be compatible. Also the perfume will generally be polar in nature.

When the composition is a water-in-oil microemulsion the perfume will,because of its lipophilic nature, form the predominant part of the oilphase. It is preferred if the perfume comprises 60% by weight or more,preferably 70% by weight or more, of the oil phase when the compositionis a water-in-oil microemulsion.

Perfumes contain a number of ingredients which may be natural productsor extracts such as essential oils, absolutes, resinoids, resins etc.and synthetic perfume components such as hydrocarbons, alcohols,aldehydes, ketones ethers, acids, esters, acetals, ketals, nitrites,phenols, etc. including saturated and unsaturated compounds, aliphatic,alicyclic, heterocyclic and aromatic compounds. Examples of such perfumecomponents are to be found in “Perfume and Flavour Chemicals” by SteffenArctander (Library of Congress catalogue card no. 75-91398).

Any lipophilic perfume which is compatible with nonionic and/or cationiccompounds may be used in the composition.

The compositions contain 15-95 wt % of lipophilic perfume, preferably20-90 wt %, more preferably 25-85 wt %, such as 40-85 wt %, e.g. 45-80wt %.

More than one lipophilic perfume may be used in the compositions of theinvention.

Dye

The dye is an at least a sparingly water-soluble dye and may be any suchdye conventionally used in softening and cleaning products. It isespecially preferred that the dye has a solubility in water of equal to,or greater than, 2 g in 100 ml of water at 20° C., preferably equal toor greater than 5 g.

The dye may be an acid-dye or other suitable type of dye. For an aciddye, the solubility may be as high as 50 g in 100 ml of water of 20° C.

The dye is present in an amount of 0.05-5 wt %, preferably 0.1-2 wt %,more preferably 0.2-1 wt %, eg 0.25-0.7 wt %.

The weight ratio of perfume to dye is preferably within the range 200:1to 5:1, more preferably 150:1 to 10:1, e.g. 100:1 to 15:1, such as 80:1to 20:1. Depending upon the amount of dye required, the ratio could betowards the lower end of the ratio e.g. 40:1 to 25:1. However if only asmall amount of dye is required the ratio may be higher e.g. 900:1 to200:1, eg. 900:1 to 250:1.

Stabilising Agent

The stabilising agent comprises a cationic stabilising agent having anLα to Lβ transition temperature of 45° C. or below for a 5 wt %dispersion of the stabilising agent in water. This Lα to Lβ transitioncan be measured by DSC as defined in “Handbook of Lipid Bilayers”, DMarsh, CRC Press, Boca Raton, Fla., 1990 (pages 137 and 337).

Any cationic stabilising agent meeting the above transition temperaturerequirement, may be used according to the invention. Compounds fallingwithin definitions of formulae (i) are (ii) below and meeting thetransition temperature requirements are cationic stabilising agentsaccording to the invention. Compounds falling within the definitions (i)and (ii) but which do meet the transition temperature requirements arenot cationic stabilising agents as herein defined.

The cationic stabilising agent used in the invention is preferably acationic surfactant, more preferably one of the quaternary ammoniumcompounds of formulae (A), (i) or (ii) below. Compounds of theseformulae are only stabilising agents as referred to herein if they meetthe above transition temperature requirement.

wherein R¹ and R² are independently C₁-C₆ alkyl, alkenyl, substitutedalkyl or alkenyl groups, or hydroxyalkyl groups and R³ and R⁴ areindependently C₈-C₂₈ alkyl, alkenyl, substituted alkyl or alkenylgroups, or hydroxalkyl groups. Preferably R¹ and R² are independentlyC₁-C₂ groups and R³ and R⁴ are independently Cl₂-C₂₂ groups, X⁻ is acompatible anion eg Cl⁻, MESO₄ ⁻, Br⁻, I⁻ acetate etc.

A cationic surfactant stabiliser according to formula (A) is ditallowyldimethyl ammonium chloride.

The cationic stabiliser may also be a compound as defined by formulae(i) and (ii) below, provided, that compound meets the transitiontemperature requirements therein defined.

A cationic stabiliser according to formula (i) below is dioleyl ester ofmethyl triethanol ammonium methosulphate wherein one R¹ is methyl andone is hydroxyethyl, both n are 2, both T are O—C═O, and both R² aretallow.

It is preferred that the stabilising agent is compatible withconventional fabric softening agents, and in particular with the fabricsoftening agents described herein. Mixtures of cationic stabilisingagents may also be included. In many cases the cationic stabilisingagent and the fabric softening agent will be the same compound.

Optional Stabilising Agent

Nonionic stabilising agents may be used in addition to the cationicstabilising agent. Preferably the nonionic stabilising agent is anonionic surfactant. Suitable types of nonionic surfactants includealcohol alkoxylates especially ethoxylates, preferably C₈-C₂₀ alkylesters alkoxylated with an average of 1 to 10 alkoxylate units,preferably 1 to 7 alkoxylate units. The ethoxylates, especiallysecondary alcohol ethoxylates, are particularly preferred.

The total amount of stabilising agent (cationic or cationic plusnonionic)in the compositions is 4 wt %-50 wt %, preferably 10-30 wt %,more preferably 15-25 wt %. Where a mixture of cationic and nonionicstabilisers are used, the weight ratio of cationic:nonionic ispreferably in the range 99:1 to 50:50, more preferably 99:1 to 60:40.

It is especially preferred that 10 wt %-30 wt % cationic surfactant isused as the stabilising agent, plus optionally an additional amount ofnonionic stabilising agent.

The weight ratio of perfume to the total amount of stabilising agent ispreferably within the range 10:1 to 1:1, more preferably 8:1 to 1:1,e.g. 5:1 to 1:1, e.g. 3:1 to 1:1.

Water-miscible Solvent

The compositions comprise water-miscible solvents in amounts of up to 10wt % of the composition, preferably up to 7.5 wt % as an essentialelement of the invention. The solvent is preferably present in an amountof 0.1-10 wt %, more preferably 0.5 to 7.5 wt %.

The water-miscible solvent may be solvent having a C₁-C₆ alkyl chainsuch as ethanol or isopropanol. The solvent may be present in thecompositions either through direct addition or it may be added by beingpresent in the stabilising agent or other component of the composition.

The compositions may also include low amounts (up to 5% by weight) of‘minor’ ingredients (other than dye or perfume) typically found infabric softening compositions, provided, the stability of thecomposition is not affected. ‘Minor’ ingredients that may be includedinclude fatty acids, non-aqueous solvents, fluorescers, hydrotropes,antifoaming agents, anti-redeposition agents, enzymes, opticalbrightening agents, opacifiers, anti-shrinking agents, anti-wrinkleagents, anti-spotting agents, germicides, fungicides, anti-oxidants, UVabsorbers (sunscreens), sequestrants, preservative, chlorine scavengers,pH buffering agents, dye fixatives, anti-corrosion agents, drapeimparting agents, and antistatic agents.

The compositions comprise 0.1-20 wt % water, preferably 0.1-15 wt %,more preferably 0.1-10 wt %.

Any suitable method of preparing the compositions of the invention maybe used. For example the perfume, stabilising agent and any other oilsoluble ingredients are mixed together to form a clear liquid. Gentleheating and/or stirring may be necessary at this point to produce theclear liquid (typically heating at 25-45° C.). Water-soluble ingredientsincluding the dye (and other ‘minor’ ingredients such as preservative)are dissolved separately in the required amount of water. Thewater-soluble aqueous portion is added to the perfume containingmixture, in aliquots if required, with stirring to produce thecomposition.

A further aspect of the present invention provides a method of producinga fabric softening composition by adding a composition of the inventionto a base composition comprising a cationic and/or nonionic fabricsoftening agent. Preferably the base composition is aqueous. Theaddition may be made in any suitable manner.

The composition is added at a suitable % by weight to give the requiredamount of perfume and dye etc. in the resultant fabric softeningcomposition. The addition amount, and effectiveness of mixing, can beeasily checked by measuring the colour. The fabric softener compositionproduced by the above method contains cationic and/or nonionic fabricsoftening agents.

Types of cationic fabric softeners that may be used in the fabricsoftening compositions produced from the compositions of the inventioninclude substantially water-insoluble quaternary ammonium materials, forexample, a compound having two C₁₂-C₂₂ alkyl or alkenyl groups connectedto a quaternary ammonium head group or a compound comprising a singlelong chain with an average chain length equal to or greater than C₂₀.Preferably these are connected to the quaternary ammonium head group viaat least one ester link.

More preferably, the invention is useful for preparing compositionscomprising quaternary ammonium material comprising a compound having twolong chain alkyl or alkenyl chains with an average chain length equal toor greater than C₁₄. Even more preferably, each chain has an averagechain length equal to or greater than C₁₆. Most preferably at least 50%of each long chain alkyl or alkenyl group has a chain length of C₁₈.

It is preferred if the long chain alkyl or alkenyl groups arepredominantly linear. The especially preferred ester-linked quaternaryammonium materials for use in the invention can be represented by theformula (i):

wherein each R¹ group is independently selected from C₁₋₄ alkyl,hydroxyalkyl or C₂₋₄ alkenyl groups; and wherein each R² group isindependently selected from C₈₋₂₈ alkyl or alkenyl groups; X⁻ is anysuitable counterion, for instance a halide, acetate or loweralkosulphate ion, such as chloride or methosulphate,

Di(tallowyloxyethyl)dimethyl ammonium chloride, available from Clariant,is especially preferred, also Di (hardened tallowyloxyethyl)dimethylammonium chloride, ex Clariant). Dioleyl ester of methyl triethanolammonium methosulphate wherein one R¹ is methyl and one is hydroxyethyl,both n are 2, both T are O—C═O, and both R² are tallow may also be used.

A second preferred type of quaternary ammonium material can berepresented by the formula (ii):

wherein R¹, n, R² and X⁻ are as defined above.

It is advantageous for environmental reasons if the quaternary ammoniummaterial is biologically degradable.

Preferred materials of this class such as 1,2 bis[hardenedtallowoyloxy]-3-trimethyl ammonium propane chloride and their method ofpreparation are, for example, described in U.S. Pat. No. 4,137,180(Lever Brothers). Preferably these materials comprise small amounts ofthe corresponding monoester as described in U.S. Pat. No. 4,137,180 forexample 1-hardened tallowoyloxy-2-hydroxy-3-trimethylammonium propanechloride.

The fabric softeners used in the compositions produced from thecompositions of the invention are not required to meet the Lα to Lβtransition temperature referred to above. Only the cationic stabilisers,which may be of formulae (i) or (ii) above, are required to have thespecified transition temperature. If compounds of these formulae areused only as a fabric softening active material, the transitiontemperature requirement does not apply.

Substantially water-insoluble fabric softening compounds are defined asfabric softening compounds having a solubility of less than 1×10⁻³ wt %in demineralised water at 20° C. Preferably the fabric softeningcompounds have a solubility of less than 1×10⁻⁴ wt %, more preferablyless than 1×10⁻⁸ to 1×10⁻⁶ wt %.

The fabric softening compositions typically contain 1-8 wt % of thefabric softening compound, and are known as dilute compositions. Theymay also contain higher amounts, such as 8-50% softening compounds inwhich case they are known as concentrates.

Nonionic fabric softeners may also be used, for example sorbitan estersand glycerol monostearate.

Further ingredients, typically minor ingredients, may be added to thefabric softener compositions produced by the method described herein.

The present invention will be exemplified by way of the followingexamples. Further examples within the scope of the invention will beapparent to the skilled person. The reference to grams of activeingredient in each example refers to the weight of each ingredient assupplied by the manufacturer used in the example.

EXAMPLE 1 Concentrated Perfume Composition

The composition below was prepared by mixing the perfume and TetranylAO-1 to form a clear liquid. Gentle warming was used. The dye and waterwere mixed to form a solution and this was added in aliquots to theperfume mixture to produce the composition.

grams of active ingredient Perfume*¹ 34.2 TETRANYL AO-1*² 10.0 Patentblue dye  2.0 (10% aqueous solution by weight) *¹SOFTLINE 2000 (exGivaudan Roure; SOFTLINE IS A TRADEMARK) *²TETRANYL AO-1 is 90% dioleylester of methyl triethanol ammonium methosulphate, 10% IPA (Ex Kao).TETRANYL is a trademark.

EXAMPLE 2 Concentrated Perfume Composition

The composition below was prepared according to the method of example 1.

grams of active ingredient Perfume*³ 34.2 AO-1*² 10.0 Patent blue dye(5%  2.0 aqueous solution by weight) *³SOFTLINE B53 ex Givaudan Roure

EXAMPLE 3 Concentrated Perfume Composition

The composition below was prepared according to the method of example 1.

grams of active ingredient Perfume*¹ 34.2 PRAPAGEN 3445*⁴ 10.0 Patentblue dye  2.0 (10% aqueous solution by weight) *⁴PRAPAGEN 3445 is 70%ditallowyl dimethyl quaternary ammonium chloride, 20% IPA and 10% water(ex Clariant). PRAPAGEN is a trademark.

EXAMPLE 4 Concentrated Perfume Composition

The composition below was prepared according to the method of example 1.

grams of active ingredient Perfume*⁵ 34.2 ARQUAD 2T*⁶ (as 12.2 supplied)RHODAMINE B dye  2.0 (5% aqueous solution by weight) *⁶cationicsurfactant ditallowyl dimethyl quaternary ammonium chloride (ex Akzo).ARQUAD is a trademark. *⁵HORIZON 2000 ex IFF. HORIZON is a trademark.RHODAMINE is a trademark.

EXAMPLE 5 Concentrated Perfume Composition

The composition below was prepared according to the method of example 1.

grams of active ingredient Perfume*⁵ 34.2 AO-1*² 10.0 Patent blue dye 2.0 (10% aqueous solution by weight)

EXAMPLE 6 Concentrated Perfume Composition

The composition below was prepared according to the method of example 1.

grams of active ingredient Perfume*³ 35.0 GENAPOL Coco 10*⁷  3.0 AOT-1*⁸ 4.6 Patent blue dye (5%  2.0 aqueous solution by weight) *⁷Genapol C-10is coconut ethoxlated alcohol with an average of 10 moles of ethoxylateper mole of fatty alcohol (ex Clariant). GENAPOL is a trademark.*⁸TETRANYL AOT-1 is 80% dioleyl ester of methyl triethanol ammoniummethosulphate, 20% dipropylene glycol solvent

Examples 1 to 6 were all stable, isotropic water-in-oil microemulsions.

EXAMPLES 7 Use of Example 1 to Prepare a Fabric Softening Composition

A fabric softening base composition comprising 94.5 parts water and 5parts dihardened tallow dimethyl ammonium chloride was prepared. To this0.5 parts of example 1 was added and the composition stirred untilhomogeneous (to provide approximately 0.37% perfume, 0.11% AO-1 and0.002% dye). A stable fabric softening composition was produced thatshowed the same physical characteristics as the comparative examplebelow.

A comparative example was produced by the conventional method of mixingtogether the following ingredients:

grams of active ingredient Dihardened tallow 5.0  dimethyl ammoniumchloride Perfume*¹ 0.3  Patent blue dye 0.002 Water to 100%

The fabric softening composition comparative example and the fabricsoftening composition produced from example 1 both exhibited goodstability on storage at room temperature.

EXAMPLE 8

A concentrated fabric conditioner was prepared from 1,2 bis[hardenedtallowoyloxy]-3-trimethyl ammonium propane chloride following standardprocedures but without perfume or dye. Subsequently the perfume dyemixture of example 2 was added to this composition with gentle stirring.The Table below shows product viscosity, measured at 106S⁻¹, as ameasure of stability compared with a control product of identicalcomposition but with perfume and dye added separately during theconditioner preparation.

24 hours old 2 weeks 4 weeks 4° C. Prototype 113  98 88 Control 114 111101  Ambient Prototype 113 103 86 Control 114 112 96 37° C. Prototype113 101 84 control 114 107 90

What is claimed is:
 1. A liquid composition comprising: (a) 15-95 wt %lipophilic perfume, (b) 0.05-5 wt % water-soluble dye, (c) about 10 wt %to about 30 wt % of a stabilising agent comprising a cationicstabilising agent that is a compound of general formula (A)

wherein R¹ and R² are independently C₁-C₆ alkyl, alkenyl, substitutedalkyl or alkenyl groups, or hydroxyalkyl groups; and R³ and R⁴ areindependently C₈-C₂₈ alkyl, alkenyl, substituted alkyl or alkenylgroups, or hydroxyalkyl groups or, a compound of general formula (i)

wherein each R¹ group is independently selected from C₁₋₄ alkyl,hydroxyalkyl or C₂₋₄ alkyl groups; and wherein each R² group isindependently selected from C₈₋₂₈ alkyl or alkenyl groups; X⁻ ischloride or methosulphate;

or, a compound of general formula (ii)

wherein R¹, n, R² and X⁻ are as defined above; and (d) water misciblesolvent; wherein the composition comprises between 0.1 to 20 wt % water,the cationic stabilising agent has an Lα to Lβ transition temperature of45° C. or below for a 5 wt % dispersion of the stabilising agent inwater and the solvent is present in an amount of up to 10 wt %.
 2. Acomposition according to claim 1 wherein the composition is an isotropicliquid.
 3. A composition according to claim 2 wherein the isotropicliquid is a water-in-oil microemulsion.
 4. A composition according toclaim 1 comprising 40-85 wt % perfume.
 5. A composition according toclaim 1 wherein the perfume has a solubility in water of equal to, orless than 0.5 g in 100 ml of water at 20° C.
 6. A composition accordingto claim 1 comprising 0.2 wt % to 1 wt % dye.
 7. A composition accordingto claim 1 wherein the dye has a solubility in water of equal to orgreater than 5 g of 100 ml of water at 20° C.
 8. A composition accordingto claim 1 wherein the weight ratio of perfume to dye is within therange 200:1 to 5:1, preferably 100:1 to 15:1.
 9. A composition accordingto claim 1 wherein the weight ratio of perfume to stabilising agent is10:1 to 1:1, preferably 5:1 to 1:1.
 10. A composition according to claim1 comprising 0.1-10 wt % water.
 11. A method of preparing a fabricsoftening composition comprising the steps; (i) preparing a basecomposition comprising a cationic and/or nonionic fabric softeningagent, and (ii) adding to (i) a composition according to claim 1, toproduce the fabric softening composition.
 12. A fabric softeningcomposition obtainable by the method of claim 11.